P
US8946305B2ActiveUtilityPatentIndex 68

Method for crosslinking a colloid, and crosslinked colloid therefrom

Assignee: LIAO CHUN-JENPriority: Dec 22, 2011Filed: Sep 10, 2012Granted: Feb 3, 2015
Est. expiryDec 22, 2031(~5.5 yrs left)· nominal 20-yr term from priority
Inventors:LIAO CHUN-JENWANG WEN-HSIYANG MING-CHIALIAO WEI-JU
B01J 13/0039
68
PatentIndex Score
5
Cited by
48
References
18
Claims

Abstract

The disclosure provides a method for crosslinking a colloid, including: (a) providing a colloid solution; (b) adding a crosslinking agent and solid particles to the colloid solution, wherein the amount of solid particles added is enough to convert the colloid solution into a solid mixture, and wherein a crosslinking reaction proceeds in the solid mixture; and (c) removing the solid particles from the solid mixture.

Claims

exact text as granted — not AI-modified
What is claimed is: 
     
       1. A method for crosslinking a colloid, comprising:
 (a) providing a colloid solution; 
 (b) adding a crosslinking agent and solid particles to the colloid solution, wherein the amount of solid particles added is enough to convert the colloid solution into a solid mixture, and wherein a crosslinking reaction proceeds in the solid mixture; and 
 (c) removing the solid particles from the solid mixture, wherein step (c) comprises washing the solid mixture with an acid to remove the solid particles and to revert the solid mixture into a crosslinked colloid, wherein the acid comprises hydrochloric acid, acetic acid, phosphoric acid or peroxy acid. 
 
     
     
       2. The method for crosslinking a colloid as claimed in  claim 1 , wherein the amount of the colloid solution is about 1-10 parts by weight, the amount of the crosslinking agent is about 0.1-5 parts by weight and the amount of the solid particles is about 5-100 parts by weight. 
     
     
       3. The method for crosslinking a colloid as claimed in  claim 1 , wherein the colloid solution is at least formed from a colloid substance and a solvent. 
     
     
       4. The method for crosslinking a colloid as claimed in  claim 3 , wherein the colloid substance comprises hyaluronic acid, collagen, chitosan, chondroitin, water soluble cellulose or polyalcohol. 
     
     
       5. The method for crosslinking a colloid as claimed in  claim 3 , wherein the solvent comprises water, alcohol, ether, ketone, benzene, ester or aldehyde. 
     
     
       6. The method for crosslinking a colloid as claimed in  claim 1 , wherein step (b) comprises:
 (i) adding the crosslinking agent to the colloid solution and mixing to start the crosslinking reaction; and 
 (ii) adding the solid particles to the colloid solution containing the crosslinking agent to convert the colloid solution into a solid mixture, wherein the crosslinking reaction is continued in the solid mixture. 
 
     
     
       7. The method for crosslinking a colloid as claimed in  claim 6 , wherein after about 1-60 minutes of performing step (i), step (ii) is performed. 
     
     
       8. The method for crosslinking a colloid as claimed in  claim 6 , wherein in step (ii), the crosslinking reaction is continued for about 1-24 hours. 
     
     
       9. The method for crosslinking a colloid as claimed in  claim 1 , wherein the crosslinking agent and solid particles are added to the colloid solution at the same time. 
     
     
       10. The method for crosslinking a colloid as claimed in  claim 9 , wherein the reaction time for the crosslinking reaction is about 1-24 hours. 
     
     
       11. The method for crosslinking a colloid as claimed in  claim 1 , wherein the crosslinking agent comprises 1,4-butanediol diglycidyl ether (BDDE), N-hydroxysuccinimide (NHS), 1-hydroxybenzotriazole (HOBt), 2-chloro-1-methylpyridinium iodide (CMPI), 2-Chloro-4,6-dimethoxy-1,3,5-triazine (CDMT), carbonyldiimidazole, octenyl succinic anhydride (OSA), methacrylic anhydride, glutaraldehyde (GTA), 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide (EDC), poly(ethylene glycol) diglycidyl ether (EX 810), ethylene sulfide, divinyl sulfone (DVS), poly(ethylene glycol)-diamine, dithiolthreitol (DTT), akyl halides or epoxides. 
     
     
       12. The method for crosslinking a colloid as claimed in  claim 1 , wherein the solid particles comprise chloride, oxide, hydroxide, fluoride, nitrate, sulfate, nitrite, ammonium salt, phosphate, silicate, carbonate particles or oxalate particles. 
     
     
       13. The method for crosslinking a colloid as claimed in  claim 1 , wherein the particle size of the solid particles is about 1-1000 μm. 
     
     
       14. The method for crosslinking a colloid as claimed in  claim 1 , after step (c), further comprising:
 (d) washing the crosslinked colloid with a base to perform a neutralization reaction. 
 
     
     
       15. The method for crosslinking a colloid as claimed in  claim 14 , wherein the base comprises sodium hydroxide, aluminum hydroxide, ammonia aqueous or alkaline hydroxide. 
     
     
       16. The method for crosslinking a colloid as claimed in  claim 14 , after step (d), further comprising:
 (e) washing the crosslinked colloid with a washing solution. 
 
     
     
       17. The method for crosslinking a colloid as claimed in  claim 16 , wherein the washing solution comprises ethyl alcohol, glycerol, neat soap, acetone, water, chloroform, dimethyl sulfoxide (DMSO), sodium hydroxide, hydrochloric acid or polyethylene glycol (PEG). 
     
     
       18. The method for crosslinking a colloid as claimed in  claim 17 , wherein a weight ratio of the crosslinked colloid to the washing solution is about 1-20:1-20000.

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